Reactions of Zr{Al(OPr i ) 4 } 2 Cl 2 or Zr{Nb(OPr i ) 6 } 2 Cl 2 with KNb(OPr i ) 6 /KAl(OPr i ) 4 and diethanolamines RN(CH 2 CH 2 OH) 2 [R ¼ H(L H H 2 ), Me(L Me H 2 ), and Ph(L Ph H 2 )] in the presence of two equivalents of Et 3 N yield interesting hetero(bi-and tri-) nuclear derivatives (1)-(8). All of these new derivatives have been characterized by elemental analyses, molecular weight measurements, and spectroscopic studies.